Process for making conducting-films.



45 to be formed (in the resent case cobalt or a mixture of cobalt'an nickel in various pro- UNITED s'rA'rEs PATENT OFFICE.

THOMAS A, EDISON, OF LLEWELLYN PARK, NEW JERSEY, ASSIGNOR TO EDISON STORAGE BATTERY COMPANY, OF WEST ORANGE, NEW JER- SEY, A CORPORATION OF NEW JERSEY.

PROCESS FOR MAKING CONDUCTING-FILMS.

Patented Kay 29, 1906.

Application filed Hay 28,1006. Serial No. 262.476.

1'0 all whom it may concern:

Be it known that l, Tnoms ALVA EnIsoN, a citizen of the United States, residing at Llewell Park, Oran e, county of Essex, and State 0 New Jersey, ve invented a certain new and useful Process for Makin Conductin -Films for Storage Batteries, o1 which the i0 owingis a description. M invention relates to a new process for dhh'wiuctln' -films ada ted particularly for'u'se fora dition to t e nickel hydroxid em loyed "in the make up of positive electrodes or storage batteries of the Edison t e. These scales or films are composed em or wholly or partly of cobalt or cobaltnickel alloy, the advantages of which are ointed out and claimed in my application or Letters Patent filed March 30, 1905, Se-

rial No. 252,935.

By the improved process it will be ossible to make use of other insoluble or re atively insoluble metals in connection with the cobalt, (such as bismuth, copper, cadmium, and iron,) the resulting compound or alloy resenting very beautiful scales or films w 'ch are eminently suited for the desired pur ose.

7 My object is to provide a simple and e ective rocess for the urpose which can be carrie out commercia ly at low cost.

To this end the invention consists in fus-- ing a sulfur compound of the metal or metals,

' the resulting fused mass being then cooled to result in the c stallization of the metallic sulfur compoun, in thin scales 0;; films, which are then separated, subsequently roasted to convert the sulfur compound into an ox gen compound of the metal or metals, an the oxygen compound thus secured is finally reduced to the metallic state in a hydrogen atmosphcre or in any other suitable way.

As a specific example of the rocess as applied to the manulacture of sea es or films of cobaltor cobalt-nickel alloy I proceed substantially as follows: I first take the oxid of the metal or metals from which the films are portionst and convert the same by the ,addition oi'sulfur in any suitable way to form the sesquisulfid of the metal or metals. The sesquisulfidthus secured is now mixed with irom six to eight times its weight with sulfid of potash or soda, (commonly called liver of &

sulfur,) and the resultin mixture is then fused in a crucible until filly liquid, or instead the metallic oxid, sulfur, and alkaline sulfid may be added together at the same time, whereby the fusion of the mass will result in the formation of the metallic sesquisulfid. The fused mass is now cooled throughout, resultlnglin the crystallization of the see-- e metalor metals,such or stals quisulfid of t ranging from .0001 to .0002 in this ess. When the ses uisulfid of two metals, such as cobalt and nic el, are thus fused and cooled, the resulting crystals will be composed of the sesquisulfid of both metals'in the proportions in which the oxids thereof were originally used. After the mass has been entirely cooled it is washed in warm water, dissolving out the potassic or sodic sulfid, leaving the scales or films, which are then dried. Generally there will be resent inthe dried mass roportion of t e sesquisulfid crystals which do not formscales or films, but which exist as very fine particles capable of being effectively separated from the usual scales or films by a screening operation through a screen about two hundred mesh. Such a screening operation is therefore performed to effect this separation, and the fine non-scaly crystals thus sepgrated are returned to the crucible and resed with a fresh batch of the mixture of sesquisulfid and the potassic or sodic sulfid. In this case, of course, the

pploper allowance should be made for the sulcontents presented by the additional increment of the fine non-scaly particles to the crucible.

Having obtained the scales or films in the form of sesquisulfid of the metal or metals desired, I now roast the same in the air to eliminate the sulfur and reoxidize the scales or films and reeonvert the latter into an oxid of the metal or metals, but without in anyway aiiecting the scale-like or crystalline. form thereof. The oxid films on scales thus ob tained are reduced to the metallic state by heat in a hydrogen atmosphere and are then ready for use.

Since both nickel and cobalt on the crystallization of their sulfids result in the production of scales or films, I am enabled to vary the proportion of the two metals in any suitable cent. of nickel are used. Furthermore, the tendenc sult in t e formation of scales or films in the manner described is so marked that it becomes possible to admix oxide of other insoluble or relatively insoluble metals thereii1-such as bismuth, copper, cadmium, or ironresulting in the formation of scales or films composed of nickel or cobalt, or both, with other metals incorporated therewith, whereby the cost of manufacture may be considerably reduced, and in some instances superior effects may be obtained.

Having now described my invention, what I claim as new therein, and desire to secure by Letters Patent, is as follows:

1. The process of makin conducting-films, which includes fusing a su fur compound of a metal or metals, in coolin the fused mass to result in the crystallization of the metallic sulfur compound in thin scales or films, in separating such scales or films, and in finally converting the latter to the metallic state, substantially as set forth.

2. The process of making conducting-films, which consists in fusing a sulfur com ound of a metal or metals, in cooling the fuse mass to result in the crystallization of the metallic sulfur compound in thin scales or films, in separating the latter, in roasting the scales or films to oxidize the same, and in finall reducin the scales or films to the metallic state, substantially as set forth.

3. The process of making conducting-films, which consists in fusing'a sulfur com ound of a metal or metals, in cooling the fuse mass to result in the crystallization of the metallic sulfur compound in thin scales or films, in separating the latter, in roasting the scales or films to oxidize the same, and in finally reducing the scales or films in a hydrogen atmosphere to the metallic state, substantially as set forth.

4. The process of making conducting-films, which includes fusing a sulfur compound of the metal or metals, in cooling the fused mass to result in the crystallization of the metallic sulfur compound in thin scales or films, in

screening t e scales or films to eliminate nonscaly crystals, and in finally reducing the scales or films to the metallic state, su'bstan-.

tially as set forth.

5. The process of making conducting-films, which includes fusing a mixture of a sulfur compound of the metal or metals with an alkaline sulfid, in cooling the fused mass to result in the crystallization of the metallic sulfur compound in thin scales or films, in removing the alkaline sulfid therefrom, and in of both nickel and cobalt to re-- finally reducing the scales or films to the metallic state, substantially as set forth;

6. The process of making conducting-films, which consists in fusin a mixture of a sulfur compound of the metafior metals with an alkaline sulfid, in cooling the fused mass to result in the crystallization of the metallic sulfur compound in thin scales or films, in removing the alkaline sulfid therefrom, in oxidizin the scales or films, and in finally reducing t e same to the metallic state, substantially as set forth.

7. The process of making conducting-films, which includes fusing a sulfur compound of cobalt, in cooling the fused mass to result in the crystallization of the sulfur compound in thin scales or films, and in finally reducing the scales or films to the metallic state, substantially as set forth.

8. The process of making conducting-films, which consists in fusin a sulfur compound of cobalt, in cooling the sod mass to result in the or stallization of the metallic sulfur compoun in thin scales or films, in oxidizing the scales or films, and in finally reducin the same to the metallic state, substantia y as set forth.

9. The process of making conducting-films, which consists in fusin a sulfur compound of cobalt, in cooling the setl mass to result in the c stallization of the metallic sulfur compoun d in thin scales or films, in roastin the scales or films to eliminate sulfur and oxidize the same, and finally in reducing the oxid to the metallic state, substantially as set forth.

10. The process of making conductingfilms, which consists in fusing a sulfur compound of cobalt, in cooling the fused mass to result in the crystallization of the metallic sulfur com ound in thin scales or films, in screening t e mass to eliminate non-scaly crystals, in roasting the scales or films to eliminate sulfur and oxidize the same, and in finally reducing the oxid to the metallic state, substantially as set forth.

11. The process of making conductingfilms, which includes fusing a mixture of a sulfur compound of cobalt and alkaline sulfid, in cooling the fused mass to result in the c stallization of the metallic compound in t 'n scales or films, in washing the mass to eliminate the alkaline sulfid, and in finally feducing the scales or films, substantially as set forth.

This specification signed and witnessed this 20th day of May, 1905. v THOS. A. EDISON.

' Witnesses:

FRANK L. DYER, MINA C. MAOARTHUR.

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